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STANDARD OPERATING PROCEDURES

SOP:
1844
PAGE:
1 of 6
REV:
0.0
DATE: 11/08/02

SOIL pH DETERMINATION
CONTENTS
1.0

SCOPE AND APPLICATION

2.0

METHOD SUMMARY

3.0

SAMPLE PRESERVATION, CONTAINERS, HANDLING AND STORAGE

4.0

INTERFERENCES AND POTENTIAL PROBLEMS

5.0

EQUIPMENT/APPARATUS

6.0

REAGENTS

7.0

PROCEDURES
7.1
7.2
7.3
7.4
7.5
7.6
7.7
7.8

pH Calibration Procedure
pH Meter Operation
Temperature Compensation
Sample Preparation with Reagent Water
Sample Preparation with Calcium Chloride Solution
Sample Measurement
Battery Replacement
Cleaning the Probe

8.0

CALCULATIONS

9.0

QUALITY ASSURANCE/QUALITY CONTROL

10.0

DATA VALIDATION

11.0

HEALTH AND SAFETY

12.0

REFERENCES

13.0

APPENDICES

STANDARD OPERATING PROCEDURES


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SOIL pH DETERMINATION
1.0

SCOPE AND APPLICATION


This standard operating procedure (SOP) describes the measurement of pH (the ratio of hydrogen [H+] and
hydroxyl [OH-] ion activities at a given temperature) of soils using a Cole-Palmer Digi-Sense digital
pH/millivolt/oxidation reduction potential (pH/mV/ORP) meter.
Mention of trade names or commercial products does not constitute United States Environmental Protection
Agency (U.S. EPA) or Lockheed Martin endorsement or recommendation for use.

2.0

METHOD SUMMARY
Measurement of soil pH using a potentiometer determines the degree of acidity or alkalinity in soils
suspended in water and in 0.01Molar (M) calcium chloride solution. The potentiometer is calibrated with
buffer solutions of known pH prior to the analysis of samples.
pH measurements are determined in both water and a calcium chloride solution because the calcium
displaces some of the exchangeable aluminum. The low ionic strength counters the dilution effect on the
exchange equilibrium by setting the salt concentration of the solution closer to that expected in the soil
solution. The pH values obtained from the measurement of the calcium chloride solution are slightly lower
than those measured in water due to the release of additional aluminum ions that hydrolyze. Therefore,
both measurements are required to fully define the character of the soil.

3.0

SAMPLE PRESERVATION, CONTAINERS, HANDLING AND STORAGE


Soil samples should be collected in wide-mouth glass containers with Teflon-lined caps. From the time of
sample collection until after analysis, samples must be refrigerated at 4 2 degrees Celsius ( C) for periods
specified by the Scientific, Engineering Response and Analytical Services (SERAS) Task Leader or the
U.S. EPA/Environmental Response Team (ERT) Work Assignment Manager (WAM). Samples must be
analyzed immediately (within 15 minutes) after the soil sample is suspended in water or calcium chloride
solution according to the procedures listed in Section 7.0. Laboratory analyses are typically performed at
room temperature (15 to 25 C). All samples and calibration buffers should be allowed to equilibrate to
ambient temperature prior to analysis.

4.0

INTERFERENCES AND POTENTIAL PROBLEMS


The combination electrode is relatively free from interference from color, turbidity, colloidal matter,
oxidants, reductants, and high salinity. Refer to pH/mV/ORP meter manufacturers instructions for any
possible interference and limitations.
Measurements of pH are affected by temperature in two ways: mechanical effects that are caused by
changes in the properties of the electrodes, and chemical effects caused by equilibrium changes. Standard
pH buffers have a specific pH at indicated temperatures.

5.0

EQUIPMENT/APPARATUS
The following are standard materials and equipment required for soil pH determination:

STANDARD OPERATING PROCEDURES


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SOIL pH DETERMINATION
pH meter, Cole-Parmer Digi-Sense Model No. 5938-00 or equivalent
Combination pH electrode
9-volt battery
Thermometer, capable of reading between 0 C and 100 C
Balance, capable of weighing 10 grams (g) of soil
No. 10 sieve, 2 millimeter (mm) openings
Small griffin beaker
pH paper
Kimwipes or equivalent
6.0

REAGENTS
pH Buffers, 4.00, 7.00 and 10.00, commercially available
Potassium chloride (KCl) solution, saturated, used for filling the combination electrode. If
separate glass and reference electrodes are used, the reference electrode is filled with
saturated aqueous KCl.
Reagent Water, distilled or deionized water, pH 6.5 to 7.5. Deionized or distilled water
should be used for rinsing the probe between samples.
Calcium Chloride Solution, 0.01M - Dilute 20.0 milliliters (mL) of stock 1.0 M calcium
chloride solution to 2 liters (L) with deionized water. The pH of this solution should be
between 5 and 7. Adjust pH of this solution if necessary.

7.0

PROCEDURES
7.1

pH Calibration Procedure
The pH/mV/ORP meter must be standardized with a known buffer solution every three hours of
operation. Refer to SERAS SOP #2077, pH/mV/ORP Determination Using a Cole-Parmer DigiSense Meter for specific calibration procedures. The buffers selected should bracket the pH of the
samples.

7.2

pH Meter Operation
Refer to SERAS SOP #2077, pH Determination Using a Cole-Parmer Digi-Sense Meter.

7.3

Temperature Compensation
Temperature compensation can be set manually by the temperature ( C) adjustment over a range
of 0 C to 100 C.

7.4

Sample Preparation with Reagent Water


1

Air dry the soil sample.

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SOIL pH DETERMINATION

7.5

7.6

Sieve the soil sample through a No. 10 sieve (2 mm mesh) to remove the coarser soil fraction.

Weigh out approximately 10 g of the air-dried and sieved soil sample.

Place the soil into a glass container and add approximately 10 mL of distilled or deionized
water.

Mix thoroughly and let stand for 1 hour.

Proceed to Section 7.6 for sample measurement.

Sample Preparation with Calcium Chloride Solution


1

Weigh out approximately 10 g of the air-dried and sieved soil sample.

Place the soil into a glass container and add approximately 10 mL of 0.01 M calcium chloride
solution.

Mix thoroughly and let stand for 1 hour.

Proceed to Section 7.6 for sample measurement.

Sample Measurement
Samples should be analyzed immediately (within 15 minutes after preparing sample in Section 7.4
or 7.5).
1

Measure the temperature of the suspended soil sample. Set the temperature dial on the pH
meter to match the measured temperature in C.

Rinse the probes with distilled or deionized water. Blot dry.

With the meter on, place the electrode in the partially settled sample suspension to be
measured.

4.

If the meter is calibrated using pH 4.00 and pH 7.00 buffers and the sample reading is >7.00,
the meter must be recalibrated using pH 7.00 and 10.00 buffers. Likewise, if the meter is
calibrated using 7.00 and 10.00 buffers and the pH reading is <7.00, the meter must be
recalibrated using the 4.00 and 7.00 buffers. The sample pH will be displayed. Record the
reading once the meter has stabilized.

Alternatively, the pH may be determined using wide range pH paper if there appears to be
interferences with the electrode from the matrix.
7.7

Battery Replacement

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SOIL pH DETERMINATION
The pH meter uses a 9-volt battery with a life of 2,000 hours. If the low battery indicator is on,
immediately stop operation and replace the internal battery with a new 9-volt battery.
7.8

Cleaning the Probe


The glass bulb is the sensitive part of the probe, it should always be kept clean. Rinse the probe
with deionized or distilled water after use. Before storage, rinse the probe with tap or distilled
water, shake dry, and place the probe in the protective cap, which should be filled with a calcium
chloride solution or equivalent probe storage solution.
If calcium chloride solution or equivalent storage solution is not available, use a 4.00 pH buffer,
7.00 pH buffer, or tap water. Distilled water should never be used.

8.0

CALCULATIONS
The value displayed is read directly as pH. The temperature of the samples and calibration buffers should
be identical to ensure accuracy. Record the sample temperature with the pH value obtained.
Report the pH of the soil to the first decimal place. Specify the medium used (water or calcium chloride)
for each pH measurement.

9.0

QUALITY ASSURANCE/QUALITY CONTROL


The following general QA procedures apply:
All data must be documented on field data sheets or in site or laboratory notebooks.
All instrumentation must be operated in accordance with the manufacturers instructions. Equipment
check-out procedures and calibration activities must be performed in Section 7.1.
Duplicate samples should be processed with the frequency of one in twenty samples. Duplicate samples
will be used to determine precision.
Ensure pH buffers are within expiration dates.
The balance used to weigh out the samples must be calibrated using a Class - S weight each time samples
are weighed out.

10.0

DATA VALIDATION
For the pH meter, 0.1 pH unit represents the limit of accuracy under normal conditions, especially for
measurement of water and poorly buffered solutions(1).
Results will be reviewed by the Engineering Evaluation Unit (EEU) prior to release. This information will
be utilized to qualify the environmental sample results accordingly with the projects data quality
objectives.

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SOIL pH DETERMINATION
11.0

HEALTH AND SAFETY


General laboratory and field safety practices should be followed. Waste samples should be handled with
care due to the uncertainty of the properties and contents involved. Refer to the specific material safety
data sheet (MSDS) for the hazardous properties of any chemical or reagent utilized in this analysis. All
excess samples, used samples, and waste material generated during analysis must be disposed in
accordance with SERAS SOP #1501, Hazardous Waste Management.
When working with potentially hazardous materials, follow U.S. EPA, Occupational Safety and Health
Association (OSHA), and Corporate health and safety procedures. More specifically, refer to SERAS SOP
#3013, Laboratory Safety Program.

12.0

REFERENCES
(1)

American Society of Testing and Materials (ASTM). 1995.


Designation D4972 - 95a: Standard Test Method for pH of Soils.
13.0

APPENDICES
This section is not applicable to this SOP.

Annual Book of ASTM Standards,